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A kind of preparation method of high-purity 5n aluminum isopropoxide

A technology of aluminum isopropoxide and isopropanol, which is applied in the field of preparation of high-purity 5N aluminum isopropoxide, can solve the problems such as the inability to use a stainless steel reactor, the inability to improve the reaction rate, the influence of product use, etc. Production cycle, efficiency improvement, effect of improving production efficiency

Active Publication Date: 2015-12-02
山东中科绿碳科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] 1. Use mercuric chloride and mercuric iodide as initiators. Although their efficiency is high, they are highly toxic, and the Hg generated during the reaction will enter the product, which will have a certain impact on the use of the product
[0004] 2. The synthesis of aluminum isopropoxide uses anhydrous aluminum trichloride as a catalyst. It is necessary to dissolve aluminum chloride in isopropanol at low temperature and then add it to the reactor. The reactor equipment has strict requirements and stainless steel reactors cannot be used. , only enamel reactors can be used
Not suitable for application in industrial production
[0006] 4. Using aluminum isopropoxide as an initiator can reduce the introduction of impurities, but the reaction rate cannot be improved

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Inject 40kg of isopropanol (AR) into the reaction kettle, add 452g of 5N aluminum isopropoxide to the isopropanol at room temperature, stir at room temperature for 5min, then add 30g of anhydrous aluminum trichloride and 160g of isopropoxide to the isopropanol Aluminum propoxide, stirring for 5 minutes;

[0030] Add 4.5kg of aluminum pellets, set reflux reaction at 85°C, the reaction initiation time is 50min, and the reaction ends in 4 hours;

[0031] Set 85°C to carry out atmospheric distillation of the above reactants to recover isopropanol;

[0032] After atmospheric distillation, the contents of the kettle were distilled under reduced pressure at 1333 Pa (absolute pressure), and fractions at 135°C-145°C were collected to obtain aluminum isopropoxide.

[0033] After testing, through the above method, the reaction is relatively fast, the yield of aluminum isopropoxide is 91.5% (relative to aluminum), and the prepared high-purity aluminum isopropoxide has a purity gre...

Embodiment 2

[0037] Inject 40kg of isopropanol (AR) into the reaction kettle, add 301g of 5N aluminum isopropoxide to the isopropanol at normal temperature, stir at room temperature for 5min, then add 20g of anhydrous aluminum trichloride and 200g of aluminum trichloride to the isopropanol, and stir 5min;

[0038] Add 6.0kg of aluminum pellets, set reflux reaction at 85°C, trigger time is 60min, and the reaction ends in 5 hours;

[0039] Set 85°C to carry out atmospheric distillation of the above reactants to recover isopropanol;

[0040] After atmospheric distillation, the contents of the kettle were distilled under reduced pressure at 1333 Pa (absolute pressure), and fractions at 135°C-145°C were collected to obtain aluminum isopropoxide.

[0041] After testing, the reaction is quicker through the above method, the yield of aluminum isopropoxide is 90.2% (relative to aluminum), and the prepared high-purity aluminum isopropoxide has a purity greater than 99.999%, meeting the quality requ...

Embodiment 3

[0043] Inject 40kg of isopropanol (AR) into the reaction kettle, add 602g of 5N aluminum isopropoxide to the isopropanol at room temperature, stir at room temperature for 5min, then add 35g of anhydrous aluminum trichloride and isopropanol to the isopropanol Aluminum 100g, stir for 5min;

[0044] Add 6.0kg of aluminum particles, set reflux reaction at 85°C, trigger time is 55min, and the reaction ends in 5 hours;

[0045] Set 85°C to carry out atmospheric distillation of the above reactants to recover isopropanol;

[0046] After atmospheric distillation, the contents of the kettle were distilled under reduced pressure at 1333 Pa (absolute pressure), and fractions at 135°C-145°C were collected to obtain aluminum isopropoxide.

[0047] After testing, the reaction is quicker through the above method, the yield of aluminum isopropoxide is 90.2% (relative to aluminum), and the prepared high-purity aluminum isopropoxide has a purity greater than 99.999%, meeting the quality require...

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Abstract

The invention discloses a preparation method of high-purity 5N aluminum isopropoxide. According to the preparation method, isopropanol and 99.996% metal aluminum are taken as raw materials and a mixture of anhydrous aluminium trichloride and 5N aluminum isopropoxide is taken as a catalyst; the preparation method is characterized in that in the preparation process, the aluminum isopropoxide is added by two steps: firstly, the aluminum isopropoxide is added for removing water from the isopropanol; secondly, the aluminum isopropoxide and the aluminium trichloride are added at the same time to function as the catalyst. Through hydrolysis reaction of the 5N aluminum isopropoxide, water in the isopropanol is consumed, so that influence of a small amount of water on the reaction and the initiator anhydrous aluminum chloride can be eliminated; after application of the 5N aluminum isopropoxide, not only is influence of water on the product purity reduced, but also the function of a cocatalyst is achieved; due to adoption of a mixed catalyst, the reaction efficiency of the isopropanol and the aluminum is improved, the production cycle is shortened, the production efficiency is improved and the cost is reduced.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, in particular to a method for preparing high-purity 5N aluminum isopropoxide. Background technique [0002] At present, the production of high-purity 5N aluminum isopropoxide (that is, aluminum isopropoxide with a mass purity of 99.999%) by the alkoxide method has been widely used. The reaction between isopropanol and aluminum is carried out, and different types of reagents are used as initiators. The initiators used here are mainly HgCl 2 , HgI 2 , anhydrous AlCl 3 , I 2 , Aluminum isopropoxide. [0003] 1. Use mercuric chloride and mercuric iodide as initiators. Although they have high efficiency, they are highly toxic, and the Hg generated during the reaction will enter the product, which will have a certain impact on the use of the product. [0004] 2. The synthesis of aluminum isopropoxide uses anhydrous aluminum trichloride as a catalyst. It is necessary to dissolve aluminum...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C31/32C07C29/70
CPCB01J31/26C07C29/70C07C29/80C07C31/32
Inventor 徐鸿
Owner 山东中科绿碳科技有限公司
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